<p>Transition metal oxide nanosheets are currently receiving significant attention due to their unique structural advantages and promising chemical and physical properties for a wide range of applications. Among them, vanadium pentoxide (V₂O₅) emerges as a highly attractive electrode material for supercapacitors, owing to its stable crystal structure and strong Faradaic activity. In this study, various microstructural characterization techniques including X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), Brunauer–Emmett–Teller (BET) surface area analysis, and spectroscopic methods such as X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) are employed to investigate the structural and surface features of the synthesized materials. Notably, V₂O₅/NiO nanocomposites exhibit a high specific surface area of 12.876 m²/g. FESEM analysis confirms the effective distribution of V₂O₅ within the NiO nanosheets, while XPS verifies the presence of vanadium (V), nickel (Ni), and oxygen (O) elements in the composite. Electrochemical measurements reveal that the nanocomposites deliver a remarkable specific capacitance of 907.567 F g⁻¹ at a current density of 1.0 A g⁻¹ and retain 84% of their initial capacitance even at 6 A g⁻¹. This study provides a valuable reference for the development of environmentally friendly thin-film electrodes aimed at high-performance energy storage devices.</p>